Characterization of Organic Matter and Hydrocarbon Potential of Shale from Uturu, Isigwuato, Se Nigeria

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1 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September Characterization of Organic Matter and Hydrocarbon Potential of Shale from Uturu, Isigwuato, Se Nigeria Uzoegbu, M.U. and Ikwuagwu, C.S. Department of Geology, Michael Okpara University of Agriculture, Umudike, PMB 7267, Umuahia, Abia State Abstract- The Cretaceous sediments in the Anambra Basin (SE Nigeria) consist of a cyclic succession of coals, carbonaceous shales, silty shales and siltstones interpreted as deltaic deposits. The HI versus Tmax and HI versus OI diagrams were used in classifying the organic matter in the shale indicating the presence of Type III kerogen. Tmax values between 426 and 439ºC indicate that the shales are thermally immature to marginally mature with respect to petroleum generation. Hydrogen Index (HI) values range from to 31.00mgHC/gTOC while S 1 + S 2 yields values ranging from 0.22 to 1.00mgHC/g rock, suggesting that the shale have gas generating potential. The TOC of shale samples of the studied Uturu locality ranges from 1.51 to 2.95%, an indication of a good to excellent source rock of terrestrially derived organic matter. The average oxygen index (OI) (8.00 mgco 2 g -1 TOC) suggest deposition in a shallow marine environment. Based on the kerogen type, shales from Uturu, Nkporo Formation have the capability of generating oil and gas if sufficient maturity attained since the studied area is part of active Cretaceous petroleum system in the Anambra Basin. Where shales are being assessed for their petroleumgenerative potential (i.e hydrocarbon source rock perspective), Rock-Eval prolysis to source rock s approach is most informative, since organic matter (OM) are solely prone to diagenetic and catagenetic transformation into liquid petroleum (i.e bitumens, crude oils, e.g. [6]. This paper aims to determine the organic matter types and their corresponding depositional environment; the quality, maturity and characterization of organic matter. 7º 8º Index Terms- Kerogen type, Organic matter, Maturity, Shale, Source rock. T I. INTRODUCTION he Anambra Basin became the site of major deposition following the Santonian folding in southeastern Nigeria. Compressional uplift of the Lower Benue Trough succession (Albian to Coniacian) along a NE-SW axis was accompanied by tectonic inversion and downwarping of the Anambra platform (Fig. 1). Estimates of total sediment thickness in the Anambra Basin from gravity measurements range from m [1], out of which between 3000 and 3500m were deposited during the late Cretaceous (Upper Campanian to Maastrichtian). At Uturu, there has not been detailed work on the shale deposit. Traditionally, organic petrographic studies are mainly used for determining coal and shale quality, composition, paleodepositional environment, or organic matter ranking [2]. Recently multi-analytical approach to organic petrography analysis uses SEM-EDS, microprobe, Rock-Eval 6 pyrolysis, solvent extract, and gas chromatography - Mass Spectrometry (GC MS) (i.e biomarkers), hydrous pyrolysis (e.g [3], [2], [4], [5]). UTURU IHUBE Fig. 1: Generalised geological map of the SE Nigeria (boxed areas of inset) showing the location of the coal deposits. Numbers indicate Cretaceous and Tertiary formations shown in Fig. 7 as follows: 1. Asu River Group; 2. Odikpani Formation; 3. Eze-Aku Shale; 4. Awgu Shale; 5. Enugu/Nkporo Shale; 6. Mamu Formation; 7. Ajali Sandstone; 8. Nsukka Formation; 9. Imo Shale; 10. Ameki Formation and 11. Ogwashi-Asaba Formation (modified from [7]). Materials and Methods A total of 6 samples were collected from Uturu. The number of samples from any of this locality was based on the accessibility of the sample area and the extent to which the shale is development at the outcrop (Plates A and B).

2 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September (a) (b) Plates a, b: Field photograph of shale outcrop at Uturu along the Okigwe- Arochukwu road. Samples Preparation For each of these samples, 30 to 50g was used for the analyses. The samples were washed to remove the dirts and sands on them. The washed samples were kept in the oven for 24 hours to dry at temperature of 40 C. The dried samples were crushed by mortar and pestle. After crushing the samples, each of these crushed samples were divided into two equal parts. Half of the crushed samples in each case was packaged in a plastic bag and the remaining half was pulverized by vibratory disc mill Model RS 100 to <50µm size. Rock-Eval 6 Pyrolysis A mass of 11 36mg of the pulverized samples were weighed in crucibles with a balance weighing instrument model Sartorius ISO The weighed samples together with the crucibles were placed in a Rock-Eval 6 machine where the samples were subjected to initial temperature of 100 C before it was increased to 300 C and finally to the temperature of 850 C. In between these temperatures, the Tmax, the temperature at maximum rate of pyrolysable (S2) hydrocarbon generation, was determined. Also free oil content (S1), pyrolysable hydrocarbon content (S2), and amount of CO 2 (S3) were determined (Fig. 2). UTTU FID Response 700 CO Response FID Response (millivolts) CO and CO2 Response (millivolts) - Temp (oc) CO2 Response Temp Profile Time (min) Fig. 2: Programmed pyrolysis result profile. Result and Discussions In shale samples, average TOC of 2.0wt% is considered an excellent source rock as HI greater than 350mgHC/gTOC is proposed to generate high commercial quantity of petroleum [8]. Highest TOC content of 2.95wt% was obtained from the shale samples from Uturu. Its values range from 1.34 to 2.95wt% with a mean of 1.85wt% (Table 1). The TOC of the shale samples range from wt% with an average of 1.85 wt% from the Uturu shale samples. The highest TOC value of 2.95 wt% was obtained from the sample number UTTU-2. The organic matter content of the UTTU-3 from the outcrop locality is quite low (1.34 wt%) compared with that of the UTTU-2 sample which has a high organic matter content. High TOC contents of >>2.95wt.% and HI between and 31.00mgHC/gTOC characterise

3 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September the shale beds of the Uturu locality. The shale have TOC contents of 1.34 to 2.95wt.% and HI values between and 31.00mgHC/gTOC. Variation in HI between and 31.00mgHC/gTOC on the shale samples, suggests Type III OM [9]. The Uturu samples are within Type III OM. Generally all the samples indicate a high contribution of OM from higher terrestrial organism (Figs 4 and 5) [10]. The S 2 values correspond to the hydrocarbons that evolve from the sample during the second programmed heating stage of pyrolysis. These hydrocarbons result from the cracking of heavy hydrocarbons and from the thermal breakdown of kerogen. It represents the milligrams of residual hydrocarbons in one gram of rock, thus indicating the potential amount of hydrocarbons that the source rock might still produce if thermal maturation continues. Samples from the Uturu locality are having their S 2 values within the range of mg/g with an average of The S 2 vs. TOC diagrams gave an average HI value of 44mgHC/gTOC for shale samples (Fig. 3). Therefore, most of the Anambra Basin shale samples were type III dominated with associated type II. The gas-prone nature of these shales (S2/S3; ) from Uturu rules out type II kerogen, which usually shows S2/S3 greater than 5 [11] (Table 1). Plots of S 2 vs. TOC and determining the regression equation of average HI of 44mgHC/gTOC has been used by [12] as the best method for determining the true average HI and measuring the adsorption of hydrocarbons by the rock matrix. They noted that HI obtained from Rock-Eval pyrolysis of shaly source rocks, in most cases, may be less than the true average HI of the sample due to the hydrocarbons adsorptive capacity of the source rock matrix [13] and that using the regression equation derived from the S 2 vs. TOC graph automatically correct HI for this effect. The average HI of the Uturu shale samples from the S 2 vs. TOC plots is very reliable (correlation coefficient is 0.95) which indicated a value of 44mgHC/gTOC (Fig. 3) which is below 300 mghc/gtoc [9], hence supporting the predominant of the type III with associated type II organic matter of the Anambra Basin. HI vs. Tmax diagram classifies the OM in the shale as type III kerogen [10]. HI values for the shale samples range from 14 to 31 mghc/gtoc and S1 + S2 yields range from 0.22 to 1.00 mghc/g rock, suggesting that the shale also have gas and oilgenerating potential as seen in Ihube [7]. [9] has suggested that at thermal maturity equivalent to vitrinite reflectance of 0.6% (Tmax 435 o C), rocks with HI above 300mgHC/gTOC produce oil; those with HI between 300 and 150 produce oil and gas; those with HI between 150 and 50 produce gas, and those with less than 50 are inert (Fig. 4). The van Krevelen diagrams for the shale samples show a dominance of type III (Fig. 4). The highest HI samples may be assigned to a high-potential type II kerogen at the diagenesis/ catagenesis boundary [13]. The corresponding HI-Tmax diagram based on the values given by [9] indicates some potential between oil and gas with gas dominating (Fig. 4). Majority of the samples fall into fields that have hydrocarbon generative potential as seen in shales from Uturu samples (Figs. 5 and 6). The Uturu samples are mixed with recycled terrestrial organic worked OM pointing to type III (Fig. 5). These recycled OM might have been

4 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September S 2 mg/g y = 0.442x R² = TOC (%) Av. HI = 44 Uturu Fig. 3: A diagram of S2 versus TOC of shale samples from Uturu with calculated average hydrogen indices (Av. HI). Type III OM, and hence to determine if the Tmax anomalies transported by fluvial processes [13], [14] as found in have prodelta shales of a delta system. The samples from Uturu were plotted on the OI vs. Tmax diagram of [15] to test if samples followed the typical trend for Fig. 4: A plot of HI versus Tmax indicating type of organic matter and maturity level Tmax ( C) GAS OIL & GAS OIL Uturu HI (S2mg/gTOC) Fig. 5: A diagram of Tmax versus HI of shale samples from Uturu describing the quality of organic matter.

5 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September any relationship to thermal conditions. The trends in Uturu shale samples show essentially a decrease in OI as Tmax increases indicating the maturity level (Table 1). This reflects the samples under study contain essentially Type III kerogen since they follow [15] typical trend for Type III OM. In the diagram Tmax vs. HI (Fig. 6) indicates that most of the OM falls into oil and gas portion which implies that the OM contains oil and gas potential. A Plot of the SOM (extract yield) against TOC as proposed by Landis and Connan (1980) in [16] for the shale samples indicates that migration of oil has taken place (Fig. 6). This diagram does not recognize the oil source rock potential of coals and coaly samples and can therefore not be used to evaluate such samples. This is supported by the diagram of S1 + S2 vs TOC (Fig. 7) characterizing the shale samples from Uturu as good to excellent source rocks with TOC and S1 + S2 of 1.85wt% and 51.0mg/g respectively. This is also supported by the report of [17] from their investigations on shaly facies of gas prone sequences in the Anambra Basin based on the values of TOC ( wt%) and soluble organic matter (SOM) ( ppm) which are indicative of fair to good and adequate source potential. [18] also investigated the Maastrichtian sediments around Enugu escarpment of the Anambra Basin which revealed the exceeding minimum threshold TOC value ( wt %) for shale samples. Thermal maturity was confirmed by plotting the profiles of Tmax vs TOC (Table 1) showing that only UTTU-4 shale sample from Uturu that did not attain to oil window Soluble Organic Matter (ppm) Migrated Oil Oil Source Rocks Non Oil Source Rocks Uturu TOC (%) Fig. 6: A diagram showing the characterization of organic matter: SOM. vs TOC [30] of samples from Anambra Basin indicating no migirated oil in the area. are low but their thermal gas generation based on Tmax vs. HI (430ºC) while the rest of samples attained to threshold indicates oil and gas potential. The observed increase in PI and value and are mature. The hydrocarbon generative capacity (S1 + S1/TOC supports the hydrocarbon generative potential of these S2) shows that the Uturu shale (0.22 to 1.00) UTTU-2 has the shale samples. highest residual potential to expel hydrocarbons as compared to the UTTU-3 sample. The thermal maturation for Uturu shale is, however, moderate. Although the S1+S2 of the locality involve Fig, 7: A diagram indicating the quality of kerogen type in the shale samples from Uturu: S1 + S2 versus TOC.

6 International Journal of Scientific and Research Publications, Volume 6, Issue 9, September ACKNOWLEDGEMENTS Gratitude is expressed to all the Staff in the Department of Geology, Michael Okpara University of Agriculture, Umudike on their advice towards the success of this work. Trican Geological Solutions, Alberta, Canada is gratefully acknowledged for the analyses of these samples. REFERENCES [1] K. O. Ladipo, C. S. Nwajide, and S. O. Akande, Cretaceous and Paleogene sequences in the Abakaliki and Anambra basins, Southeastern Nigeria. Nat. Symp. on Geology of deltas, [2] G. H. Taylor, M. Teichmuller, A. Davis, C. F. K. Diessel, R. Littke, and P. Robert, Organic Petrology. Gebruder Borntraeger, 1998, p [3] M. G. Fowler, F. Goodarzi, I. Gentais, and P. W. Brooks, Hydrocarbon potential of middle and upper Devonian coals from Meville Island, Arctic Canada. Org. Geochem., vol. 17, p , [4] H. I. Petersen, A reconsideration of the oil window for humic coal and kerogen Type III. J. Petrol. Geol., vol. 25, p , [5] R. Walker, and M. Mastalerz, Functional group and individual maceral chemistry of high volatile bituminous coals from southern Indiana: Controls on coking. Intern. J. Coal Geol., vol. 58, p , [6] H. I. Petersen, Morphology, formation and paleoenvironmental implications of naturally formed char particles in coals and carbonaceous mudstones Fuel, vol.77, p , [7] S. O. Akande, I. B. Ogunmoyero, H. I. Petersen, and H. P. Nytoft, Source rock evaluation of coals from the Lower Maastrichtian Mamu Formation, SE Nigeria. J. Petrol. Geol., vol. 30 no.4, p , [8] B. P. Tissot, and D. H. Welte, Petroleum Formation and Occurrence, 2 nd Ed. Springer- Verlag, Berlin, Heidelberg, New York, Tokyo, p. 699, [9] K.E. Peters, Guidelines for evaluating petroleum source rocks using programmed pyrolysis. Am. Assoc. Petrol. Geol. Bull., vol. 70, p , [10] A. Bechtel, H. J, Gawlick, R. Gratzer, M. Tomaselli, and W. Puttmann, Molecular indicators of palaeosalinity and depositional environment of small scale basins within carbonate platforms: The Late Triassic Hauptdolomite Wiestalstausee section near Hallein (Northern Calcareous Alps, Austria). Org. Geochem., vol. 38, p , [11] E. Eseme, R. Littke, and C. M. Agyingi, Geochemical characterization of a Cretaceous black shale from Mamfe Basin, Cameroon. Petrol. Geosci., vol. 12, p , [12] F. F. Langford, and M. M. Blanc- Valleron, Interpreting Rock-Eval pyrolysis data using graphs of pyrolyzable hydrocarbons vs Total Organic Carbon. Am. Assoc. Petrol. Geol. Bull., vol. 74 no.6, p , [13] N. G. Obaje, H. Wehner, G. Scheeder, M. B. Abubakar, and A. Jauro, Hydrocarbon prospectivity of Nigeria s inland basins: From the viewpoint of organic geochemistry and organic petrology. Am. Assoc. Petrol. Geol. Bull., vol. 88 no.3, p , [14] M. I. Bird, R. E. Summons, M. K. Gagan, Z. Roksandic, L. Dowling, J. Head, L. K. Fifield, R. G. Cresswell, and D. P. Johnson, Terrestrial vegetation change inferred from n-alkanes 13C analysis in the marine environment. Geochemica. Cosmochim. Acta., vol. 59, p , [15] P. Landis, M. Monthious, and J. D. Meunier, Importance of the oxidation/maturation pair in the evolution of humic coals. Org. Geochem., vol. 7, p , [16] B. Jovancicevic, H. Wehner, G. Scheeder, K. Stojanovic, A. Sainovic, O. Cvetkovic, M. Ercegovac, and D. Vitorovic, Search for source rocks of the crude oils of the Drmno deposition (southern part of the Pannonian Basin, Serbia). J. Serbian Chem. Soc., 67, , [17] F. Beka, V. Ukaegbu, O. Oluwajana, N. Oledinma, I. Njoku, J. Beka, L. Amaechi, and M. Udoh, Spatial profiling of shaly facies and palaeoenvironment reconstruction of gas prone sequences in the Anambra Basin, Nigeria. Nig. Assoc. Petrol. Expl. 25 th Annual Conf., Abuja, Nigeria. Abs. vol., p. 25, [18] G. G. Udofia, and I. M. Akaegbobi, Integrated geochemical and organic petrographic characterization of the Campano-Maastrichtian sediments around Enugu Escarpment, Anambra Basin, Southeastern Nigeria. Nig. Assoc. Petrol. Expl. 25 th Annual Conf., Abuja, Nigeria. Abs. vol., p. 22, AUTHORS First Author M. U. Uzoegbu is with Department of Geology, Michael Okpara University of Agriculture, Umudike, PMB 7267, Umuahia, Abia State ( muuzoegbu@gmail.com). Second Author C. S. Ikwuagw is with Department of Geology, Michael Okpara University of Agriculture, Umudike, PMB 7267, Umuahia, Abia State ( Samchibs33@gmail.com).

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